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Tung oil-based modified amine curing agent and preparation method and application thereof

A curing agent and modified amine technology, applied in coatings, anti-corrosion coatings, epoxy resin coatings, etc., can solve the problems of easy occurrence of micro-cracks, infiltration of corrosive media, and reduced impact resistance in materials, and achieve curing reaction. Wide and uniform distribution of joints, moderate reaction speed, and excellent adhesion

Active Publication Date: 2021-08-17
INST OF CHEM IND OF FOREST PROD CHINESE ACAD OF FORESTRY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, in recent years, a large number of equipment corrosion has occurred in the harsh environment of high salt spray, high humidity and heat in marine areas, which reflects that traditional epoxy anti-corrosion coatings generally have the disadvantages of high brittleness and poor impact toughness.
In the process of long-term use, due to the influence of aging degree, alternation of temperature, and alternation of humidity, the material is prone to microcracks, which leads to the decline of its impact resistance and the penetration of corrosive media. Therefore, polyamide curing agent, cardanol The use of phenalkamine curing agent is gradually restricted
The general toughening method directly leads to the decline of the strength of the cured epoxy resin and the medium resistance such as oil resistance, so it is of great significance to develop a curing agent for epoxy resin with high anti-corrosion performance and high impact toughness.

Method used

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  • Tung oil-based modified amine curing agent and preparation method and application thereof
  • Tung oil-based modified amine curing agent and preparation method and application thereof

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0015] The first step: 146g of tung, 51.7 g of phenol and 0.438 g of toluenesulfonic acid were added to 500 ml of four round bottom flasks, and the mixture was stirred and stirred and warmed to 90 ~ 120 ° C, After the reaction was continued at 2 to 3 hours, it was naturally cooled to room temperature, and 5 wt.% NaOH aqueous solution was added to the saturated brine and washed 3 times, and the upper layer brown viscous liquid was taken after anhydrous sodium sodium sulfate. Methyl ester - phenol addition 189.3 g.

[0016] Step 2: 154.4.4 g of methyl tunne-phenol addition, adding 46.4 g of hexanediamine to 500 mL of three round bottom flasks, mixed with mixed stirring, add 37 wt.% Of formaldehyde aqueous solution 32.4 g, temperature control No more than 60 ° C, warmed up to 85 to 95 ° C after the addition was added, and after 3 to 4 h, the resulting water-proof Tongl Manis alkali curing agent was 203.2 g.

[0017] Step 3: In the stirring state, it continues to add 51.04 g of dipyon...

Embodiment 2

[0019] The first step: 146g of tantate 146g, cresol 59.4g and H 3 PO 4 0.438 g added to 500 ml of four round bottom flasks, continuously introduced into nitrogen, start stirring and warmed to 90 to 120 ° C, continued to react at 2 to 3 hours at this temperature, naturally cooled to room temperature, successively added 5 wt The aqueous solution of NaOH was washed with saturated brine and allowed to lay out 3 times, and the upper layer brown viscous liquid was taken with anhydrous sodium sodium sulfate after drying with sodium sodium sodium sulfate. 197.6 g.

[0020] Step 2: 160.0 g of methyl tunne-cresol addition, 41.2 g of divinisin 41.2 g into 500 mL of three round bottom flasks, mixed with mixed stirring, 0.8.8 g, temperature control After over 60 ° C, the temperature was raised to 85 to 95 ° C, and after 3 to 4 h, it was removed, and the formed water was distilled off, and the resulting water-proof Tongyekanis alkali curing agent was 219.3 g.

[0021] Step 3: In the stirring st...

Embodiment 3

[0023] The first step: 146g of methyl tunnes, 82.5 g and AlCl of t-butylphenol 3 0.438 g added to 500 ml of four round bottom flasks, continuously introduced into nitrogen, start stirring and warmed to 90 to 120 ° C, continued to react at 2 to 3 hours at this temperature, naturally cooled to room temperature, successively added 5 wt .% NaOH aqueous solution and saturated brine were washed and staveted for 3 times, and the upper layer brown viscous liquid was taken with anhydrous sodium sodium sodium sulfate. Dry tunnesyl phenol was added 217.6 g.

[0024] Step 2: Methyl tunkate - 176.8 g of tert-butyl phenol, 58.4 g of Trivadic tetraamine, 58.4 g of Trivadic Tetramine, and mixed with isobutyldereide, and 0.8.8 g of isobutyl is mixed. The temperature control did not exceed 60 ° C. After the addition was added, the temperature was warmed to 85 to 95 ° C, and after 3 to 4 h, it was removed, and the resulting water-proof Tongl Manis alkali curing agent 250.2 g was removed.

[0025] St...

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Abstract

The invention discloses a tung oil-based modified amine curing agent and a preparation method and application thereof, the preparation method comprises the following steps: adding methyl eleostearate, phenol and a catalyst into a reaction container, under the state of continuously introducing nitrogen, stirring and heating for reaction, then cooling, washing and standing, taking an upper brown viscous liquid, and drying with anhydrous sodium sulfate to obtain a tung oil source phenol adduct; adding the tung oil source phenol adduct and polyamine into a reaction container, uniformly mixing and stirring, dropwise adding aldehyde, heating to react after dropwise adding, and carrying out reduced pressure distillation to remove generated water so as to obtain the tung oil-based Manny base curing agent; and under a stirring state, continuously dropwise adding polyamine into the tung oil-based Manny base curing agent, carrying out heating reflux, then carrying out an amidation reaction, stopping heating when no water and free amine are evaporated out, and cooling to room temperature to obtain the dark brown viscous tung oil-based modified amine curing agent. The tung oil-based modified amine curing agent has wider and more uniform curing reaction activity crosslinking point distribution, and can well balance the hardness and flexibility of the coating so that the coating is more tough.

Description

Technical field [0001] The present invention belongs to the field of thermosetting resin material, and more particularly to a tung oil-based modified amine curing agent and a preparation method thereof. Background technique [0002] The epoxy resin / curing agent system has good workability, due to an epoxy group containing a very large active epoxy group, a hydroxyl group, an ether bond, an amine bond, an ester bond, and its own higher cohesive force to an epoxy curing. Higher adhesive strength, in addition, has good dimensional stability, low shrinkage, excellent electrical insulation, high mechanical strength, good solvent resistance, can be used as castings, laminate, adhesive, coating and the like. The curing agent acts on the performance of epoxy resin preservative coatings, so a suitable curing agent must be selected. The polyamide curing agent and the epoxy resin can be cured at normal temperature, and the coating film has good anti-corrosion, flexibility and removal; the...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G59/62C09D163/00C09D5/08C08G14/12
CPCC08G59/623C09D163/00C09D5/08C08G14/12C09D7/63C08K5/0025
Inventor 李梅杨小华夏建陵张燕丁海阳李守海诸进华陈瑶
Owner INST OF CHEM IND OF FOREST PROD CHINESE ACAD OF FORESTRY
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